Supergravity continuous foam separation device and method

Abstract

The invention discloses a supergravity continuous foam separation device and method, and belongs to the technical field of chemical separation. The device comprises n supergravity rotating packed beds and (n + 1) foam columns, when n is equal to 2, the device comprises first and second supergravity rotating packed beds and first, second and third foam columns; a gas inlet of the first supergravity rotating packed bed and a gas inlet of the first foam column are simultaneously connected with a gas conveying pipeline, and a foam outlet of the first foam column is connected with a liquid outlet of the first supergravity rotating packed bed; a gas inlet of the second foam column is connected with a gas outlet of the first rotating packed bed, and a foam outlet of the second foam column is connected with a gas inlet of the second supergravity rotating packed bed; a gas inlet of the third foam column is connected with a gas outlet of the second supergravity rotating packed bed; a liquid inlet of the first rotating packed bed is simultaneously connected with a liquid outlet of the second rotating packed bed and a liquid conveying pipeline. According to the invention, efficient separation of target substances is realized, and the method is suitable for a continuous operation process.

Description

Technical Field

[0001] The invention relates to a supergravity continuous foam separation device and method, belonging to the technical field of chemical separation. Background Art

[0002] Foam separation is based on the principle of interfacial chemical surface adsorption. It uses foam or bubbles as carriers, and uses the adsorption effect of surface-active components (ions, molecules, colloidal particles, solid particles or suspended particles) on the foam surface to adhere to the rising bubble surface and then float on the liquid surface, so as to separate surfactant components or components that can combine with surfactants from the solution, thereby achieving the purpose of purifying the solution. This method has the advantages of simple equipment, mild operation, low energy consumption, high efficiency, continuous or intermittent operation, and easy industrial scale-up. It has been widely used in the fields of metallurgy, environmental protection, food, and biological separation. At present, the traditional foam separation process has problems such as large and uneven bubbles, poor stability, slow mass transfer efficiency, and low separation efficiency. Therefore, reducing the bubble size, improving the bubble morphology, and improving the mass transfer efficiency and separation efficiency are currently urgent issues to be solved.

[0003] Chinese patent CN116585757A discloses a foam separation device with an octagonal pyramid internal component containing sieve holes and its application. The invention is to purify and separate the β-glucosidase fusion protein by means of enhanced foam drainage. Experiments show that the device improves the enrichment ratio, but the recovery rate needs to be improved. Chinese patent CN103142664A discloses a method for extracting total saponins of bupleurum from bupleurum by a two-stage foam separation method. The invention involves a process of continuous foam separation of total saponins of bupleurum; and the device performs two-stage foam separation on saponins, and its separation efficiency still has potential and room for improvement. Chinese patent CN115634781A discloses a new foam separation and purification device with several porous tower plates with sieve holes added to the foam section, which extracts the surfactant wastewater sodium dodecyl sulfate (SDS) aqueous solution. The results show that the recovery rate of SDS is 97.79% and the enrichment ratio is 1.791. The design of this equipment focuses on optimizing the foam drainage process, resulting in the failure to achieve a simultaneous improvement in recovery rate and enrichment ratio, reflecting that the performance of the equipment still needs to be further balanced and optimized in these two aspects.

[0004] At present, the two key factors affecting foam separation efficiency are surface adsorption and foam drainage. In the entire foam separation process, strengthening the surface adsorption process is the core of improving separation efficiency. Some existing inventions can improve the separation effect to a certain extent by changing the property parameters of the system (such as liquid viscosity, surface tension) and optimizing operating conditions (such as gas-liquid ratio, bubble generation rate), but it is difficult to achieve a better level. In order to solve the above problems, the present invention proposes a supergravity continuous foam separation device and method. Summary of the invention

[0005] In view of the problems existing in the current foam separation technology, such as large bubbles, slow mass transfer efficiency, low separation efficiency, etc., the present invention provides a high-gravity continuous foam separation device and method.

[0006] The present invention proposes to improve the traditional foam separation equipment. Based on the principle of enhanced separation of gas-liquid two-phase in the supergravity field, a supergravity continuous foam separation device is invented. The core device is a rotating packing bed, which generates a centrifugal field through high-speed rotation to quickly separate the foam and liquid phases, aiming to strengthen the surface adsorption process, optimize the generation and rupture process of bubbles, and use the supergravity field to greatly increase the renewal rate of the gas-liquid interface, significantly improve the mass transfer efficiency and separation effect, and achieve continuous and efficient separation of target substances. The innovative points of the present invention are: ① Applying supergravity technology to the field of foam separation, providing a supergravity continuous foam separation device; using supergravity technology can greatly enhance the interface adsorption and separation process, can effectively improve the gas-liquid mass transfer efficiency, in the supergravity field, the high-speed rotating packing generates a huge shear force, the liquid is torn into a micro-liquid state after multiple times, and quickly contacts with the gas, accelerating the gas-liquid surface renewal frequency and the degree of liquid turbulence, increasing the effective contact area of ​​the target substance at the gas-liquid interface, and greatly improving the interphase mass transfer rate. ② The present invention introduces two-stage or multi-stage supergravity technology to provide two or more gas-liquid two-phase contact sites, so that the gas-liquid two-phase can be sheared and reorganized multiple times under the action of centrifugal force, which greatly accelerates the gas-liquid surface renewal rate, achieves the purpose of strengthening the surface adsorption process, increases the effective gas-liquid contact area, and significantly improves the separation and purification effect of the target substance.

[0007] The present invention provides a high-gravity continuous foam separation device, comprising n high-gravity rotating packing beds and n+1 foam columns; the present invention takes n=2 as an example to illustrate as follows: The separation device comprises a first high gravity rotating packed bed and a second high gravity rotating packed bed, a first foam column, a second foam column and a third foam column; The gas inlet of the first supergravity rotating packed bed is connected to the gas inlet of the first foam column and the gas delivery pipeline at the same time, and the foam outlet of the first foam column is connected to the liquid outlet of the first supergravity rotating packed bed; the gas inlet of the second foam column is connected to the gas outlet of the first rotating packed bed, and the foam outlet of the second foam column is connected to the gas inlet of the second supergravity rotating packed bed; the gas inlet of the third foam column is connected to the gas outlet of the second supergravity rotating packed bed; the liquid inlet of the first rotating packed bed is connected to the liquid outlet and the liquid delivery pipeline of the second rotating packed bed at the same time; The gas delivery pipeline is composed of a fan, a gas buffer tank, a gas valve, and a gas flow meter connected in sequence; the liquid delivery pipeline includes a raw material liquid tank, a pump, a liquid valve, and a liquid flow meter connected in sequence.

[0008] Furthermore, the core components of the first supergravity rotating packed bed and the second supergravity rotating packed bed are the same. The first supergravity rotating packed bed includes a rotor, a packing, a shell, a motor, and a liquid distributor. A gas inlet is provided on the lower side of the shell, a liquid inlet and a foam outlet are provided on the top, and a liquid outlet is provided on the bottom. Various packings are installed in the rotor, and the bottom of the rotor is connected to the motor and driven to rotate by the motor. The liquid delivery pipeline sprays the liquid to the inner edge of the packing through the liquid distributor. The structure of the second supergravity rotating packed bed is the same as the above structure of the first supergravity rotating packed bed. In addition, the liquid inlet of the second supergravity rotating packed bed is connected to the diverter valve under the defoamer, and the reflux liquid is transported to the inside of the packing through the liquid distributor. A guide tube is provided at the gas inlet of the second supergravity rotating packed bed to prevent excessive liquid from flowing into the second foam column and affecting the rise of bubbles. A one-way valve is provided at the liquid outlet of the second supergravity rotating packed bed, and the liquid that has not been separated by foam continues to enter the first rotating packed bed. Furthermore, the guide cylinder includes an upper cylinder and a lower cylinder, both of which are hollow conical structures, and the outer sides of which are composed of a plurality of drainage baffles with arc-shaped protrusion structures connected in sequence to form a cylindrical structure. The upper cylinder and the lower cylinder are placed at an angle, and the two are combined into a structure that is narrow at both ends and wide in the middle, and the top opening of the upper cylinder is larger than the bottom opening of the lower cylinder. Specifically, each drainage baffle occupies 1 / 4 to 1 / 36 of the circumference of the guide tube. Under the action of centrifugal force, when the splashed liquid hits the upper tube, the raised part on the drainage baffle will drain the liquid into the groove between the two drainage baffles and flow along the direction of the groove, so that the originally concentrated fluid is dispersed to different groove directions by the impact force, changing the flow direction of the liquid. The lower tube is used to block the remaining liquid in the packing bed to prevent the liquid from entering the second foam column; under the action of the guide tube, the liquid flows into the first rotating packing bed along the liquid outlet, which is conducive to the stable operation of the second foam column and prevents liquid impact; the overall height of the guide tube is set according to the size of the ultra-gravity rotating packing bed and the foam column, the height ratio of the upper tube and the lower tube is between 1:2 and 1:10, the upper tube is inclined at an angle of 5° to 85° to the vertical direction, and the lower tube is inclined at an angle of 0° to 85° to the vertical direction.

[0009] Furthermore, the foam column bodies of the first foam column, the second foam column and the third foam column are in a closed cylindrical shape; a flow guide pipe is provided on the side of the third foam column, and its outlet is connected to the defoamer. A reflux pipe is provided under the defoamer, and the defoaming liquid flows into the second supergravity rotating packing bed through the reflux pipe; another reflux pipe of the defoamer is connected to the product tank; whether to reflux, as well as the reflux time, number of cycles and reflux flow rate are determined according to product quality.

[0010] Furthermore, the guide tube structure of the third foam column is an annular tube, which is arranged on the side of the third foam column with an inclination angle ranging from 10° to 90°, and the outlet end is connected to the defoamer. The structure of the defoamer is as follows: the body of the defoamer is cylindrical, and an ultrasonic rod is installed on one side of the interior, and the ultrasonic rod extends into the interior to break the foam; a needle-shaped defoamer is arranged at the bottom and the side, and the needle-shaped defoamer is a mace-shaped structure with sharp thorns arranged upward; the ultrasonic rod and the needle-shaped defoamer can be used simultaneously or separately, and the size of the needle-shaped defoamer is determined according to the size of the defoamer; a liquid level meter is placed on the top to monitor the foam generation rate and liquid level changes in real time. If the liquid level exceeds the set value, the feed flow rate or operating conditions need to be adjusted to avoid foam overflow caused by excessive liquid; a diverter valve is arranged below the defoamer, and the diverter valve can be adjusted manually or automatically through a controller to accurately control the reflux rate of the defoaming liquid; Furthermore, a one-way valve is arranged below the second supergravity rotating packed bed to control the one-way flow of the fluid and prevent the backflow of the liquid.

[0011] Furthermore, the liquid outlet on the side of the first foam column is connected to the residual liquid tank.

[0012] Furthermore, the packing of the supergravity rotating packing bed is at least one or more combinations of ball ring packing, wire mesh packing, spherical packing, arc saddle packing, honeycomb packing, and the type of packing can be replaced. Furthermore, the packing is composed of a multi-stage rotating packing bed in series or a combination of multiple packing layers; a combination of multiple packing layers refers to arranging packings of the same or different types or specifications in sequence to form multiple independent working layers, and the function and action point of each layer of packing are different; a multi-stage rotating packing bed in series refers to a multi-stage packing formed by connecting multiple independent rotating packing beds in series in sequence, and each rotating packing bed serves as an independent processing unit.

[0013] Furthermore, through the combined design of a rotating packed bed and a foam column consisting of multi-stage series or multi-layer packings, as well as an adjustable feed, gas-liquid ratio and reflux system, efficient separation and enrichment of target substances in a continuous or semi-continuous mode are achieved; the foam column has a height-to-diameter ratio ranging from 5 to 50 and is designed according to the liquid flow rate and bubble diffusion characteristics to improve the gas-liquid contact efficiency and reduce the equipment pressure drop.

[0014] The present invention provides a supergravity continuous foam separation method. In the above-mentioned supergravity continuous foam separation device, a raw material liquid is foamed by a first supergravity rotating packed bed to generate a foam phase and a liquid phase. The foam phase passes through a gas outlet of the first rotating packed bed through a second foam column and enters a second rotating packed bed for foaming again. Under the action of the gas, the foam continuously rises and enters a third foam column, and a high-concentration target substance is obtained in a defoamer; the liquid phase in the defoamer flows back to the second rotating packed bed for continued foaming, and the remaining liquid phase flows into the first rotating packed bed for continued foam separation, and the remaining liquid phase component is obtained at the bottom of the first foam column.

[0015] Furthermore, the above-mentioned high gravity continuous foam separation method specifically comprises the following steps: (1) Start the motor and set the rotation speed of the first supergravity rotating packed bed and the second supergravity rotating packed bed. The raw material liquid is driven by the pump and injected into the first supergravity rotating packed bed after being measured by the rotor flowmeter. At the same time, start the fan to supply gas to the system. After the gas passes through the buffer tank, the gas velocity is stabilized by adjusting the flowmeter. The gas pipeline is divided into two branches: one pipeline enters the first foam column through the gas distributor and rises to the first supergravity rotating packed bed; the other pipeline directly enters the first supergravity rotating packed bed; (2) The two gases merge in the first high-gravity rotating packed bed; in the first high-gravity rotating packed bed, the liquid is thrown from the inside of the packing to the outside under the action of centrifugal force, and contacts with the gas to generate microbubbles; part of the liquid flows into the first foam column through the liquid outlet of the first rotating packed bed, and the bubbles formed at this time continue to rise to the first high-gravity rotating packed bed to achieve foam separation; (3) The foam enters the second foam column from the gas outlet of the first high-gravity rotating packed bed, and continues to rise to the second high-gravity rotating packed bed for continuous foaming. At the same time, it undergoes the process of foaming, reorganization, breaking and reorganization. The surface is constantly renewed, which effectively improves the material enrichment efficiency. During the rising process of the foam, part of the liquid it carries will flow through the liquid outlet of the second rotating packed bed to the first high-gravity rotating packed bed due to gravity for re-circulation and separation. (4) The foam in the second foam column rises into the second rotating packed bed, and continuously foams under the action of gas and rises into the third foam column, and is finally collected in the defoamer through the drainage pipe; (5) In the defoamer, bubbles are broken by ultrasonic rods or needle-shaped defoamers to form defoaming liquid. The liquid level meter at the top monitors the foam generation rate and liquid level changes in real time. A diverter valve is installed at the bottom of the defoamer to control the diversion ratio of the reflux liquid and the defoaming liquid, so that part of the defoaming liquid flows into the product tank and the other part flows back to the second rotating packed bed. After the entire separation process is completed, the product tank collects the product, and the remaining residual liquid is collected by the residual liquid tank.

[0016] In the above method, the gas-liquid contact mode is one of cross-flow, counter-flow or parallel flow, the hypergravity factor is 5-120; the gas is at least one or more of air, carbon dioxide, nitrogen, oxygen or inert gas.

[0017] In the above separation method, the reflux ratio of the defoaming liquid, the height of the foam column and the height of the packing are determined according to the foam rising speed, the gas-liquid flow rate and the separation effect; that is, the reflux ratio is controlled by controlling factors such as the gas flow rate, the liquid flow rate, the raw material liquid concentration, pH, etc., and finally the appropriate reflux speed is selected during operation to ensure that this process can be operated continuously or semi-continuously.

[0018] Beneficial effects of the present invention: (1) The present invention applies supergravity technology to the field of foam separation, significantly increases the gas-liquid contact area, and realizes efficient adsorption of the target substance on the submillimeter microbubble interface, effectively overcoming the shortcomings of traditional foam separation equipment, such as large and uneven bubbles, low mass transfer efficiency and low separation efficiency, and realizes efficient separation of the target substance; (2) The present invention utilizes an ultra-gravity continuous foam separation device to provide a two-stage or multi-stage gas-liquid two-phase contact separation site. Bubble recombination and fragmentation are performed alternately, and the surface is continuously renewed, which significantly enhances the separation effect, improves the stability of the foam and the separation efficiency. It is also suitable for continuous operation processes, is green and efficient, has low energy consumption, and meets the needs of industrial production. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 This is a schematic structural diagram of the ultra-gravity continuous foam separation device of the present invention; Figure 2 is a structural diagram of the first foam column in the device of the present invention; Figure 3 is a structural diagram of a second foam column in the device of the present invention; Figure 4 is a structural diagram of a third foam column in the device of the present invention; Figure 5 This is a diagram showing the internal structure of the first high gravity rotating packed bed in the device of the present invention; Figure 6 This is a diagram showing the internal structure of the second high gravity rotating packed bed in the device of the present invention; Figure 7 The figure is a diagram showing the internal structure of the defoamer in the device of the present invention; Figure 8 for Figure 7 Top view of the internal structure of the middle defoamer; Fig. 9 It is a three-dimensional structural diagram of the guide tube of the present invention; Fig.10 for Fig. 9 A top view of the middle guide tube; Fig.11 for Fig. 9 A plan side view of the middle guide tube; Fig.12 This is a diagram showing the internal structure of a rotating packed bed consisting of multiple layers of packing in Example 3.

[0020] In the figure: 1, raw liquid storage tank; 2, pump; 3, liquid valve; 4, liquid flow meter; 5, first supergravity rotating packed bed; 6, first motor; 7, fan; 8, gas buffer tank; 9, gas valve; 10, gas flow meter; 11, residual liquid tank; 12, first foam column; 13, second foam column; 14, second supergravity rotating packed bed; 15, second motor; 16, one-way valve; 17, third foam column; 18, liquid level meter; 19, ultrasonic disperser; 20, defoamer; 201, ultrasonic rod; 21, diverter valve; 22, product tank; 1201, first foam column gas inlet; 1202, first foam column residual liquid outlet; 1203, first foam column foam outlet; 1204, gas distributor; 1301, second foam column gas inlet; 1302, second foam column foam outlet; 170 1. Gas inlet of the third foam column; 1702. Draft tube; 1703. Foam outlet of the third foam column; 501. Gas inlet; 502. Liquid inlet; 503. Second liquid inlet; 504. Gas outlet; 505. Liquid outlet; 506. Liquid distributor; 507. Packing; 1401. Gas outlet of the second supergravity rotating packed bed; 1402. Liquid inlet of the second supergravity rotating packed bed; 1403. Liquid outlet of the second supergravity rotating packed bed; 1404. Gas inlet of the second supergravity rotating packed bed; 1405. Liquid distributor of the second supergravity rotating packed bed; 1406. Packing of the second supergravity rotating packed bed; 1407. Draft tube; 23. Liquid inlet of the rotating packed bed composed of multiple layers of packing; 24. Honeycomb packing; 25. Ball ring packing; 26. Wire mesh packing. DETAILED DESCRIPTION

[0021] The present invention is further illustrated by the following examples, but is not limited to the following examples. Example 1

[0022] like Figures 1 to 11 As shown, a supergravity continuous foam separation device includes two supergravity rotating packing beds and three foam columns in this embodiment; specifically, it includes a first supergravity rotating packing bed 5, a second supergravity rotating packing bed 14; a first foam column 12, a second foam column 13, and a third foam column 17; the second foam column 13 connects the first supergravity rotating packing bed 5 with the second supergravity rotating packing bed 14; the first foam column 12 is connected below the first supergravity rotating packing bed 5; and the third foam column 17 is connected above the second supergravity rotating packing bed 14.

[0023] like Figure 1As shown, the gas inlet 501 of the first supergravity rotating packed bed is connected to the gas delivery pipeline at the same time as the first foam column gas inlet 1201, and the first foam column foam outlet 1203 is connected to the first supergravity rotating packed bed liquid outlet 505; the second foam column gas inlet 1301 is connected to the gas outlet 504 of the first rotating packed bed, and the second foam column foam outlet 1302 is connected to the second supergravity rotating packed bed gas inlet 1404; the third foam column gas inlet 1701 is connected to the second supergravity rotating packed bed gas outlet 1401; the liquid inlet 502 of the first rotating packed bed is connected to the liquid delivery pipeline, and the second liquid inlet 503 is connected to the second supergravity rotating packed bed liquid outlet 1403; The gas delivery pipeline is composed of a blower 7, a gas buffer tank 8, a gas valve 9 and a gas flow meter 10 connected in sequence; The liquid delivery pipeline includes a raw material liquid storage tank 1, a pump 2, a liquid valve 3 and a liquid flow meter 4 which are connected in sequence.

[0024] Furthermore, the first supergravity rotating packed bed 5 includes a rotor, a packing 507, a shell, a first motor 6, and a liquid distributor 506. A gas inlet 501 (connected to a gas delivery pipeline) is provided on the lower side of the shell, a liquid inlet 502, a second liquid inlet 503 and a foam outlet 504 are provided on the top, and a liquid outlet 505 is provided on the bottom; various packings 507 are installed in the rotor, and the bottom of the rotor is connected to the first motor 6 and is driven to rotate by the first motor 6; the gas outlet 504 of the first rotating packed bed 5 is connected to the second foam column gas inlet 1301, and its liquid outlet 505 is connected to the first foam column foam outlet 1203; the liquid inlet 502 is connected to the liquid delivery pipeline, and the second liquid inlet 503 is connected to the second supergravity rotating packed bed liquid outlet 1403, so that the liquid is transported to the inside of the packing through the liquid distributor 506.

[0025] Furthermore, the internal structure of the second supergravity rotating packed bed 14 is the same as that of the first supergravity rotating packed bed 5, and the side of the lower part of the shell is provided with a second supergravity rotating packed bed gas inlet 1404 and a second supergravity rotating packed bed liquid outlet 1403; the top is provided with a second supergravity rotating packed bed liquid inlet 1402; the rotor is equipped with a second supergravity rotating packed bed filler 1406, and the bottom of the rotor is connected to the second motor 15 and driven to rotate by the second motor 15; the second supergravity rotating packed bed gas outlet 1401 is connected to the third foam column gas inlet 170 1, the second supergravity rotating packed bed liquid outlet 1403 is connected to the second liquid inlet 503 of the first supergravity rotating packed bed 5 through a one-way valve 16; the second supergravity rotating packed bed liquid inlet 1402 is connected to the diverter valve 21 below the defoamer 20, and the reflux liquid is transported to the inside of the second supergravity rotating packed bed packing 1406 through the second supergravity rotating packed bed liquid distributor 1405; a guide tube 1407 is set at the second supergravity rotating packed bed gas inlet 1404 to prevent excessive liquid from flowing into the second foam column and affecting the rise of bubbles.

[0026] Furthermore, the guide tube 1407 is a baffle of innovative design, which includes an upper tube and a lower tube. Both the upper tube and the lower tube are hollow conical structures, and the outer side thereof is composed of a plurality of drainage baffles with arc-shaped protrusion structures connected in sequence to form a cylindrical structure. The upper tube and the lower tube are placed at an angle, and the two are combined into a structure with narrow ends and a wide middle, and the top opening of the upper tube is larger than the bottom opening of the lower tube. Specifically, each drainage baffle occupies 1 / 4 to 1 / 36 of the circumference of the guide tube. Under the action of centrifugal force, when the splashed liquid hits the upper tube, the raised part on the drainage baffle will drain the liquid into the groove between the two drainage baffles and flow along the direction of the groove, so that the originally concentrated fluid is dispersed to different groove directions by the impact force, changing the flow direction of the liquid. The lower tube is used to block the remaining liquid in the packing bed to prevent the liquid from entering the second foam column 13; under the action of the guide tube 1407, the liquid flows into the first supergravity rotating packing bed 5 along the liquid outlet, which is conducive to the stable operation of the second foam column and prevents liquid impact; the overall height of the guide tube is set according to the size of the supergravity rotating packing bed and the foam column, the height ratio of the upper tube and the lower tube is between 1:2 and 1:10, the upper tube is inclined at an angle of 5° to 85° to the vertical direction, and the lower tube is inclined at an angle of 0° to 85° to the vertical direction.

[0027] Furthermore, the foam column includes a first foam column 12, a second foam column 13, and a third foam column 17; the foam column body is in a closed cylindrical shape; a flow guide tube 1702 is provided on the side of the third foam column 17, and its outlet is connected to the defoamer 20, a reflux pipe is provided below the defoamer, and a diverter valve 21 is provided on the reflux pipe to control the flow rate, and the defoaming liquid is introduced from the liquid inlet 1402 of the second supergravity rotating packing bed through a reflux pipe; the other reflux pipe is connected to the product tank 22; the gas inlet 1201 of the first foam column is connected to the gas delivery pipe, and the foam outlet 1203 of the first foam column is connected to the liquid outlet 505 of the first rotating packing bed; the second foam column 13 is connected to the gas outlet 504 of the first supergravity rotating packing bed 5 and the gas inlet 1404 of the second supergravity rotating packing bed respectively above and below; the gas inlet 1701 of the third foam column is connected to the gas outlet 1401 of the second supergravity rotating packing bed 14, and the foam outlet 1703 of the third foam column is connected to the defoamer 20.

[0028] Furthermore, the structure of the flow guide 1702 is as follows: it is located on the side of the third foam column 17, with an inclination angle ranging from 10° to 90°, and the outlet is connected to the defoamer 20; the structure of the defoamer 20 is as follows: the body of the defoamer is cylindrical, and an ultrasonic device (i.e., an ultrasonic rod) is installed on one side of the interior, and the ultrasonic rod 201 extends into the interior to break the foam; a needle-shaped defoamer is arranged at the bottom and the side, and the needle-shaped defoamer is a mace-shaped structure with sharp thorns arranged upward; the ultrasonic rod and the needle-shaped defoamer can be used simultaneously or separately, and the needle-shaped defoamer The size of the defoamer is determined by the size of the defoamer; a liquid level meter 18 is placed on its top to monitor the foam generation rate and liquid level changes in real time, and adjust the feed flow or operating conditions through feedback control to avoid foam overflow caused by excessive liquid; a diverter valve 21 is set under the defoamer 20, and the diverter valve can be adjusted manually or automatically through a controller to accurately control the reflux rate of the defoaming liquid; a one-way valve 16 is set on the liquid outlet 1403 pipeline of the second supergravity rotating packed bed to control the one-way flow of the fluid and prevent liquid backflow.

[0029] Furthermore, the residual liquid tank 11 is connected to the liquid outlet 1202 on the side of the first foam column 12 .

[0030] Furthermore, the fillers 507 of the first high gravity rotating packed bed and the fillers 1406 of the second high gravity rotating packed bed are at least one or more combinations of ball ring fillers, wire mesh fillers, spherical fillers, arc saddle fillers, and honeycomb fillers, and the types of fillers can be replaced.

[0031] Furthermore, the height-to-diameter ratio of the foam column ranges from 5 to 50 and is designed based on the liquid flow rate and bubble diffusion characteristics to improve the gas-liquid contact efficiency and reduce the pressure drop of the equipment.

[0032] The present invention provides a supergravity continuous foam separation method. In the above-mentioned supergravity continuous foam separation device, the raw material liquid is foamed by the first supergravity rotating packed bed 5 to generate a foam phase and a liquid phase. The foam phase passes through the gas outlet 504 of the first rotating packed bed through the second foam column 13 and enters the second supergravity rotating packed bed 14 for re-foaming. Under the action of the gas, the foam continuously rises and enters the third foam column 17, and a high-concentration target substance is obtained in the defoamer 20; the liquid phase in the defoamer enters the second supergravity rotating packed bed 14 due to the action of gravity to continue foaming, and the remaining liquid phase enters the first supergravity rotating packed bed 5 to continue foam separation, and the remaining liquid phase component is obtained at the bottom of the first foam column.

[0033] The above-mentioned method for high-gravity continuous foam separation comprises the following steps: Start the first motor 6 and the second motor 15 and set the rotation speeds of the first supergravity rotating packed bed 5 and the second supergravity rotating packed bed 14. The raw material liquid is driven by the pump 2 and injected into the first supergravity rotating packed bed 5 after being measured by the liquid flow meter 4. At the same time, start the fan 7 to supply gas to the system. After the gas passes through the buffer tank 8, the gas velocity is stabilized by adjusting the gas flow meter 10. The gas pipeline is divided into two branches: one pipeline enters the first foam column 12 through the gas distributor 1204 and rises to the first supergravity rotating packed bed 5; the other pipeline directly enters the first supergravity rotating packed bed 5; the two branches The gas streams converge in the first supergravity rotating packed bed 5; in the first supergravity rotating packed bed, the liquid is thrown from the inside of the packing to the outside by the centrifugal force, and contacts with the gas to generate microbubbles; part of the liquid flows into the first foam column 12 through the liquid outlet 505 of the first supergravity rotating packed bed 5, and the bubbles formed at this time continue to rise into the first supergravity rotating packed bed 5 to achieve foam separation; the foam enters the second foam column 13 from the gas outlet 504 of the first supergravity rotating packed bed, and continues to rise to the second supergravity rotating packed bed 14 to continuously foam, and at the same time undergoes foaming, recombination, During the processes of breaking and reorganizing, the surface is constantly renewed, which effectively improves the material enrichment efficiency. During the rising process of the foam, part of the liquid it carries will flow through the second high-gravity rotating packed bed liquid outlet 1403 to the first high-gravity rotating packed bed 5 for recirculation and separation. The foam in the second foam column 13 rises into the second high-gravity rotating packed bed 14, and continuously foams and rises into the third foam column 17 under the action of gas, and is finally collected in the defoamer 20 through the drainage tube 1702. In the defoamer 20, the bubbles are broken in the defoamer by the ultrasonic rod 201 or the needle-shaped defoamer. A defoaming liquid is formed; the liquid level meter 18 at the top monitors the foam generation rate and liquid level changes in real time, and adjusts the feed flow or operating conditions through a feedback mechanism to prevent foam overflow; a diverter valve 21 is installed at the bottom of the defoamer 20, which can be adjusted manually or automatically to accurately control the reflux speed of the defoaming liquid; the diverter valve on the outlet pipe of the defoamer 20 is adjusted to control the diversion ratio of the reflux liquid and the defoaming liquid, so that a part of the defoaming liquid flows into the product tank 22, and the other part flows back to the second supergravity rotating packed bed 14; after the entire separation process is completed, the product tank 22 collects the product, and the remaining residual liquid is collected by the residual liquid tank 11.

[0034] In the above method, the gas-liquid contact mode is one of cross-flow, counter-flow or parallel flow, the hypergravity factor is 5-120; the gas is at least one or more of air, carbon dioxide, nitrogen, oxygen or inert gas.

[0035] In the above separation method, a more reasonable defoaming liquid reflux system and operating conditions should be set up, and factors such as foam separation efficiency, operating stability, energy consumption and product quality should be comprehensively considered. The reflux ratio of the defoaming liquid ranges from 0 to 100%. It can be fully refluxed or the reflux time, cycle number and reflux flow rate can be determined based on product quality to keep the defoaming liquid fully foaming in the rotating packed bed and the gas-liquid mixing efficiency.

[0036] (1) Full reflux (reflux ratio 100%) is applicable to scenarios where the concentration of the target substance in the wastewater is low (for example, the protein concentration is less than 100 mg / L), and the enrichment ratio needs to be increased through multiple cycles. The target substance is difficult to desorb from the gas-liquid interface and requires a longer foam residence time. The gas-liquid ratio is generally 5:1~8:1, and the reflux flow rate is 100% of the feed flow rate.

[0037] (2) Partial reflux (reflux ratio 20%~80%) is applicable to scenarios where the concentration of target substances in wastewater is medium (for example, protein concentration is 100~300 mg / L), and the product quality requirements are high, but a certain degree of wastewater discharge is allowed. The foam enrichment ability is strong, but energy consumption and operational stability need to be taken into account. The reflux ratio of 20%~80% can be optimized through step-by-step experiments. Under common conditions, it is recommended to start from 50%.

[0038] (3) No reflux (reflux ratio 0%) is applicable when the target substance concentration in the wastewater is high (for example, the protein concentration exceeds 300 mg / L) and the foam generation rate is high, so the recovery target can be achieved without multiple cycles. The gas-liquid ratio can be maintained at 3:1~5:1 without additional reflux.

[0039] Generally, the reflux time should be shorter than the equipment processing cycle to ensure the smoothness of continuous operation. By installing a liquid level meter, the foam generation rate and liquid level change of the defoaming liquid can be monitored. Combined with the foam generation rate, the reflux time is adjusted until the system reaches a stable state. The height of the foam column and the height of the packing are determined according to the foam rising speed, gas-liquid flow rate and separation effect. Finally, the appropriate operating conditions are selected during operation to ensure that this process can be operated continuously or semi-continuously.

[0040] The separation efficiency of foam separation technology is evaluated by the enrichment ratio E and the recovery rate R: Recovery rate: Enrichment ratio: In the formula, C f Indicates the concentration of target substance in the collected defoaming solution (mg / L), C 0 represents the initial concentration of the target solute in the feed solution (mg / L), C wIndicates the concentration of target substance in the residual liquid (mg / L); V w represents the residual liquid volume (L), V 0 represents the volume of the raw material solution (L). V f Indicates the volume of defoaming solution (L).

[0041] In order to make the above-mentioned purpose of the present invention more intuitive, the specific implementation methods of the technical solution of the present invention are described in detail below in conjunction with specific embodiments. Example 2

[0042] The experiment used a simulated surfactant wastewater sodium dodecylbenzene sulfonate (SDBS) aqueous solution as the system, with an SDBS concentration of 300 mg / L. The experiment was a continuous operation, and the wastewater treatment volume was 8 L each time; the surfactant wastewater was pumped in through the liquid inlet 502 of the first supergravity rotating packed bed, with a gas velocity of 600 L / h, a feed flow rate of 450 mL / min, a supergravity factor of 40, a reflux ratio of 50%, and an experimental temperature maintained at 25°C. The operation time was 30 min, and the experiment was stopped when the foam no longer bulged, the foam entered the product tank 22, and the remaining liquid entered the residual liquid tank 11 for collection.

[0043] Finally, it was concluded that the recovery rate of SDBS in this embodiment was 95.98%, the enrichment ratio was 77, and the separation effect was good. Under the conditions of reflux ratios of 20%, 50%, and 80%, the corresponding reflux flow rates were set to 60 mL / min, 150 mL / min, and 240 mL / min, respectively. Example 3

[0044] The source of this experiment is soybean whey wastewater from a soybean product production factory. The soybean whey wastewater contains a large amount of organic matter, including COD (chemical oxygen demand) of 1500 mg / L and nitrogen content of 80 mg / L. Direct discharge will cause environmental pollution. Figure 1 ), effectively recovering proteins and other surfactants in wastewater, while reducing the pollution load of wastewater. Among them, the height-to-diameter ratio of the foam separation column is 6:1, and the filler height is 1 / 3 of the column height.

[0045] Experimental steps: Soybean whey wastewater was filtered through a 100-mesh filter to remove large suspended solids; based on the study of the effects of initial pH, bubble size, superficial gas velocity, feed concentration and foam layer height on the foam separation of soybean protein wastewater, SDS was used as a capture agent and foaming agent, and the mass concentration was added to the solution according to the standard ratio. Subsequently, 4 L of wastewater was passed into the ultra-gravity continuous foam separation device, and the gas pipeline system was started to adjust the gas velocity; it was operated at normal pressure for 30 minutes, and the surfactant in the wastewater was enriched on the bubble surface, and the generated foam was recovered by the top collector. The collected foam formed a defoaming liquid in the defoamer, and finally vacuum freeze-dried to obtain a high-concentration protein product; the treated wastewater was discharged from the bottom outlet for subsequent analysis; the foam was collected every 60 seconds, weighed and the volume of the foam liquid was recorded.

[0046] Finally, the optimal separation conditions were determined. The experimental temperature was maintained at 25°C (controlled by a water bath), the whey protein concentration was 200 mg / L, the pH was 6.2, the first supergravity factor was 45, the second supergravity factor was 30, the gas velocity was 50 L / h, the feed flow rate was 300 mL / min, the operation time was 25 min, and the experiment was stopped when the foam no longer bulged. The foam entered the product tank 22, and the remaining liquid entered the remaining liquid tank 11 for collection. Finally, the total recovery rate of soy whey protein in this embodiment was 94.5%, the enrichment ratio was 80, and the separation effect was good; the wastewater pollutant removal effect COD removal rate was 75% (reduced from 1500 mg / L to 375 mg / L), and the nitrogen content was reduced by 40% (reduced from 80 mg / L to 48 mg / L). When the reflux ratio was 50%, the foam enrichment ratio reached the optimal value of 80; when the reflux ratio was lower than 20%, the foam stability decreased; when it was higher than 80%, the foam was diluted too much.

[0047] By using this device to treat soybean whey wastewater, not only can high value-added substances such as protein be efficiently recovered, but also the pollutant concentration of wastewater can be significantly reduced. This method is easy to operate and has low operating costs, providing an efficient solution for the resource utilization of soybean whey wastewater. Example 4

[0048] The soy whey wastewater from the soy product production factory is treated by a super gravity continuous foam separation device composed of multiple layers of fillers. The height-to-diameter ratio of the foam column is 6:1. The rotating filler bed is made of high-strength corrosion-resistant materials. Its height is determined by the height of the filler and is divided into three layers (such as Fig.12As shown in the figure, the lower layer of filler is honeycomb filler 24, which promotes the initial mixing of gas and liquid and increases the foam generation rate; the middle layer of filler is ball ring filler 25, which increases the turbulence effect, strengthens the gas-liquid mass transfer and improves the separation efficiency; the upper layer of filler is wire mesh filler 26, which enhances the stability of microbubbles, prolongs the foam residence time and significantly improves the enrichment ratio; the height of each layer of filler accounts for 1 / 3 of the total height of the filler bed, and the fillers are separated by stainless steel partitions. Each layer is provided with a liquid inlet to ensure uniform distribution of the liquid. The wastewater mainly contains protein and other surfactants, with an initial COD of 1500 mg / L and a protein concentration of 200 mg / L. During the experiment, the supergravity factor was set to 50, the reflux ratio was adjustable, the feed flow rate was 300 mL / min, the gas flow rate was 50L / h (air), and the temperature was 25°C (controlled by water bath thermostat). The operation time was 30 minutes, and the defoaming liquid reflux ratio was 50%. The protein concentration of the foam liquid was measured every 5 minutes, and the foam liquid volume and wastewater treatment volume were recorded.

[0049] The experimental results show that the height of the foam column is stable at 20 cm, and the foam liquid concentration reaches 800 mg / L, which is 4 times the initial protein concentration of the wastewater; the COD reduction rate is 72.33%, that is, from 1500 mg / L to 415 mg / L. The total recovery rate is 90.5%. The enrichment ratio is 70, indicating that the device has good enrichment capacity. The ultra-gravity continuous foam separation device composed of multi-layer fillers achieves efficient protein enrichment and effective purification of wastewater by optimizing the filler structure and gas-liquid contact mechanism, and is suitable for promotion and application in soy product wastewater treatment and other biological separation fields.

[0050] For matters not covered in the embodiments of the present invention, those skilled in the art can select from the prior art.

[0051] The above disclosure is only a specific implementation of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art can easily conceive of changes or substitutions within the technical scope disclosed in the present invention, which should all be included in the protection scope of the present invention.

Claims

1. A super gravity continuous foam separation device, characterized in that: It comprises n ultra-gravity rotating packing beds and n+1 foam columns; the foam columns and the ultra-gravity rotating packing beds are sequentially connected to form a separation device; When n=2, the separation device includes a first high-gravity rotating packed bed and a second high-gravity rotating packed bed, a first foam column, a second foam column, and a third foam column; The gas inlet of the first supergravity rotating packed bed is connected to the gas inlet of the first foam column and the gas delivery pipeline at the same time, and the foam outlet of the first foam column is connected to the liquid outlet of the first supergravity rotating packed bed; the gas inlet of the second foam column is connected to the gas outlet of the first rotating packed bed, and the foam outlet of the second foam column is connected to the gas inlet of the second supergravity rotating packed bed; the gas inlet of the third foam column is connected to the gas outlet of the second supergravity rotating packed bed; the liquid inlet of the first rotating packed bed is connected to the liquid outlet and the liquid delivery pipeline of the second rotating packed bed at the same time; The gas delivery pipeline consists of a fan, a gas buffer tank, a gas valve and a gas flow meter connected in sequence; the liquid delivery pipeline includes a raw material liquid tank, a pump, a liquid valve and a liquid flow meter connected in sequence.

2. The ultra-gravity continuous foam separation device according to claim 1, characterized in that: The core components of the first supergravity rotating packed bed and the second supergravity rotating packed bed are the same. The first supergravity rotating packed bed includes a rotor, a packing, a shell, a motor, and a liquid distributor. A gas inlet is provided on the lower side of the shell, a liquid inlet and a foam outlet are provided on the top, and a liquid outlet is provided on the bottom. Various packings are installed in the rotor, and the bottom of the rotor is connected to the motor and driven to rotate by the motor. The liquid delivery pipeline sprays the liquid to the inner edge of the packing through the liquid distributor. The structure of the second supergravity rotating packed bed is the same as the above structure of the first supergravity rotating packed bed. In addition, the liquid inlet of the second supergravity rotating packed bed is connected to the diverter valve under the defoamer, and the reflux liquid is transported to the inside of the packing through the liquid distributor. A guide tube is arranged at the gas inlet of the second supergravity rotating packed bed to prevent excessive liquid from flowing into the second foam column and affecting the rise of bubbles. A one-way valve is provided at the liquid outlet of the second supergravity rotating packed bed, and the liquid that has not been separated by foam continues to enter the first rotating packed bed.

3. The ultra-gravity continuous foam separation device according to claim 2, characterized in that: The guide cylinder includes an upper cylinder and a lower cylinder, both of which are hollow conical structures, and the outer sides of which are connected in sequence by a plurality of drainage baffles with arc-shaped protrusions to form a cylindrical structure. The upper cylinder and the lower cylinder are placed at an angle, and the two are combined into a structure with narrow ends and a wide middle, and the top opening of the upper cylinder is larger than the bottom opening of the lower cylinder.

4. The ultra-gravity continuous foam separation device according to claim 3, characterized in that: Each drainage baffle occupies 1 / 4~1 / 36 of the circumference of the guide tube. Under the action of centrifugal force, when the splashed liquid hits the upper tube, the raised part on the drainage baffle will drain the liquid into the groove between the two drainage baffles and flow along the direction of the groove, so that the originally concentrated fluid is dispersed to different groove directions by the impact force, changing the flow direction of the liquid. The lower tube is used to block the remaining liquid in the packing bed to prevent the liquid from entering the second foam column; under the action of the guide tube, the liquid flows into the first rotating packing bed along the liquid outlet, which is conducive to the stable operation of the second foam column and prevents liquid impact; the overall height of the guide tube is set according to the size of the ultra-gravity rotating packing bed and the foam column, the height ratio of the upper tube and the lower tube is between 1:2~1:10, the upper tube is inclined at an angle of 5°~85° to the vertical direction, and the lower tube is inclined at an angle of 0°~85° to the vertical direction.

5. The ultra-gravity continuous foam separation device according to claim 1, characterized in that: The foam column bodies of the first foam column, the second foam column and the third foam column are in a closed cylindrical shape; a flow guide pipe is arranged on the side of the third foam column, and its outlet is connected to the defoamer. A reflux pipe is arranged under the defoamer, and the defoaming liquid flows into the second supergravity rotating packing bed through the reflux pipe; another reflux pipe of the defoamer is connected to the product tank; whether to reflux, the reflux time, the number of cycles and the reflux flow rate are determined according to the product quality; the liquid outlet on the side of the first foam column is connected to the residual liquid tank.

6. The ultra-gravity continuous foam separation device according to claim 5, characterized in that: The guide tube structure of the third foam column is an annular tube, which is arranged on the side of the third foam column with an inclination angle ranging from 10° to 90°, and the outlet end is connected to the defoamer; the structure of the defoamer is as follows: the body of the device is cylindrical, and an ultrasonic rod is installed on one side of the interior, and the ultrasonic rod extends into the interior to break the foam; a needle-shaped foam breaker is arranged at the bottom and the side, and the needle-shaped foam breaker is a mace-shaped structure with sharp thorns arranged upward; the ultrasonic rod and the needle-shaped foam breaker can be used simultaneously or separately, and the size of the needle-shaped foam breaker is determined according to the size of the defoamer; a liquid level meter is arranged at the top thereof for real-time monitoring of the foam generation rate and liquid level changes. If the liquid level exceeds the set value, the feed flow rate or operating conditions need to be adjusted to avoid foam overflow caused by excessive liquid; a diverter valve is arranged below the defoamer, and the diverter valve can be adjusted manually or automatically through a controller to accurately control the reflux rate of the defoaming liquid; the height-to-diameter ratio of the foam column ranges from 5 to 50.

7. The ultra-gravity continuous foam separation device according to claim 1, characterized in that: The filler of the ultra-gravity rotating packed bed is at least one or more combinations of ball ring fillers, wire mesh fillers, spherical fillers, arc saddle fillers, and honeycomb fillers, and the type of filler can be replaced.

8. The ultra-gravity continuous foam separation device according to claim 7, characterized in that: The packing is composed of a multi-stage rotating packing bed connected in series or a plurality of packing layers; a combination of multiple packing layers refers to arranging the packings of the same or different types or specifications in sequence to form a plurality of independent working layers, and the function and action point of each layer of packing are different; a multi-stage rotating packing bed connected in series refers to a multi-stage packing formed by connecting a plurality of independent rotating packing beds in series in sequence, and each rotating packing bed serves as an independent processing unit.

9. A high gravity continuous foam separation method, using the high gravity continuous foam separation device according to any one of claims 1 to 8, characterized in that: The raw material liquid is foamed by the first supergravity rotating packed bed to generate a foam phase and a liquid phase. The foam phase passes through the gas outlet of the first rotating packed bed through the second foam column and enters the second rotating packed bed for further foaming. Under the action of the gas, the foam continues to rise and enters the third foam column, and a high-concentration target substance is obtained in the defoamer; the liquid phase in the defoamer flows back to the second rotating packed bed to continue foaming, and the remaining liquid phase flows into the first rotating packed bed to continue foam separation, and the remaining liquid phase component is obtained at the bottom of the first foam column.

10. The high gravity continuous foam separation method according to claim 9, characterized in that The following steps are involved: (1) Start the motor and set the rotation speed of the first supergravity rotating packed bed and the second supergravity rotating packed bed. The raw material liquid is driven by the pump and injected into the first supergravity rotating packed bed after being measured by the rotor flowmeter. At the same time, start the fan to supply gas to the system. After the gas passes through the buffer tank, the gas velocity is stabilized by adjusting the flowmeter. The gas pipeline is divided into two branches: one pipeline enters the first foam column through the gas distributor and rises to the first supergravity rotating packed bed; the other pipeline directly enters the first supergravity rotating packed bed; (2) The two gases merge in the first high-gravity rotating packed bed; in the first high-gravity rotating packed bed, the liquid is thrown from the inside of the packing to the outside under the action of centrifugal force, and contacts with the gas to generate microbubbles; part of the liquid flows into the first foam column through the liquid outlet of the first rotating packed bed, and the bubbles formed at this time continue to rise to the first high-gravity rotating packed bed to achieve foam separation; (3) The foam enters the second foam column from the gas outlet of the first high-gravity rotating packed bed, and continues to rise to the second high-gravity rotating packed bed for continuous foaming. At the same time, it undergoes the process of foaming, reorganization, breaking and reorganization. The surface is constantly renewed, which effectively improves the material enrichment efficiency. During the rising process of the foam, part of the liquid it carries will flow through the liquid outlet of the second rotating packed bed to the first high-gravity rotating packed bed due to gravity for re-circulation and separation. (4) The foam in the second foam column rises into the second rotating packed bed, and continuously foams under the action of gas and rises into the third foam column, and is finally collected in the defoamer through the drainage pipe; (5) In the defoamer, bubbles are broken by ultrasonic rods or needle-shaped defoamers to form defoaming liquid. The liquid level meter at the top monitors the foam generation rate and liquid level changes in real time. A diverter valve is installed at the bottom of the defoamer to control the diversion ratio of the reflux liquid and the defoaming liquid, so that part of the defoaming liquid flows into the product tank and the other part flows back to the second rotating packed bed. After the entire separation process is completed, the product tank collects the product, and the remaining residual liquid is collected by the residual liquid tank; In the above method, the gas-liquid contact mode is one of cross-flow, counter-flow or parallel flow, the hypergravity factor is 5-120; the gas is at least one or more of air, carbon dioxide, nitrogen, oxygen or inert gas.

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